CN103031757A - Black water-based color paste for acrylic stock solution coloring and preparation method of black water-based color paste - Google Patents
Black water-based color paste for acrylic stock solution coloring and preparation method of black water-based color paste Download PDFInfo
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Abstract
The invention discloses black water-based color paste for acrylic stock solution coloring, and a preparation method of the black water-based color paste. The black water-based color paste prepared by the method takes carbon black after oxidation treatment as a pigment, the disadvantage of poor surface hydrophilicity of the common carbon black is avoided, a butyl sodium naphthalene sulfonate salt and 2-naphthalene sulfonic acid methanal polymer sodium salt composite dispersing agent system is used cooperatively, and a pigment surface treating agent, a cosolvent, sodium thiocyanate, bactericide and deionized water are taken as common ingredients, wherein the dispersing agent is mixed by butyl sodium naphthalene sulfonate salt and 2-naphthalene sulfonic acid methanal polymer sodium salt at a mass ratio of 1:(2-5). The obtained black water-based color paste for the acrylic stock solution coloring has the characteristics of small particle size and high stability in an acrylic spinning stock solution, and blocking of a spinneret orifice and greater chromatic aberration do not appear in a spinning process.
Description
Technical field
The present invention relates to a kind of original liquid coloring use mill base and preparation method thereof, relate in particular to a kind of acrylic fibers original liquid coloring with black water mill base and preparation method thereof, belong to the mill base preparation field.
Background technology
Original liquid coloring namely in the spinning solution of chemical fibre, adds colouring agent and carries out the method that coloured chemical fibre is directly made in spinning.The colored fibre color aberration of this technology preparation is little, light fastness is high, the more important thing is the chemical fibers dyeing link of having omitted the downstream, to reducing the chemical fibers dyeing cost and promoting that the effect of energy-saving and emission-reduction is fairly obvious, has good development prospect.
When adopting the sodium sulfocyanate wet spinning technology to make color acrylic fibre, the aqueous color paste of using for original liquid coloring requires high, in case cause the generation of pigment agglomeration because granules of pigments disperses insufficient in spinning solution, the situation that spinneret orifice, color differ will occur stopping up.The equipment that brings for fear of colour changing simultaneously cleans and the problem such as excessive color fiber waste, and single batch of output of color acrylic fibre is often with hundreds of tons of notes, and the output of black acrylic fibers is higher.Therefore how to reduce the acrylic fibers original liquid coloring with the particle diameter of mill base, improve its stability, strengthen itself and the excellent compatibility of stoste, reduce simultaneously it and in Polyacrylonitrile Fiber Spinning Solution, reunite, avoid stopping up the critical problem that spinneret orifice, the not first-class problem of minimizing fiber color have just become to prepare acrylic fibers original liquid coloring use mill base.
Because the carbon blacksurface lipophile is stronger, it is bad dispersibility in water, cause the less stable of carbon black color paste in Polyacrylonitrile Fiber Spinning Solution, and at present commonly used passing through carries out surface modification to carbon black, increases its easily disperse, reduces its tendency of reuniting and become one and prepare comparatively reliably the acrylic fibers original liquid coloring with the scheme of black water mill base.
The surface oxidation of carbon black and be well known to those skilled in the art by the technology that surface oxidation increases the carbon black easily disperse has not yet to see report but how to utilize carbon black after the oxidation to prepare the acrylic fibers original liquid coloring with the black water mill base.
Summary of the invention
For overcoming above-mentioned technological deficiency, the invention provides a kind of acrylic fibers original liquid coloring black water mill base and preparation method thereof, it is little that the black water mill base that the method prepares gained has a particle diameter, the high characteristics of stability in Polyacrylonitrile Fiber Spinning Solution, and spinneret orifice and the large phenomenon of aberration can not appear stopping up during spinning.
The present invention for the technical scheme that solves its technical problem and adopt is:
A kind of acrylic fibers original liquid coloring black water mill base is comprised of the carbon black after oxidation processes, surface of pigments finishing agent, dispersant, cosolvent, sodium sulfocyanate, bactericide and deionized water,
Wherein said carbon black after oxidation processes accounts for 20.0 ~ 40.0% of this black water mill base gross mass,
Described surface of pigments finishing agent is 0.02 ~ 0.04:1 with the mass ratio of carbon black after oxidation processes,
Described dispersant is 0.1 ~ 0.3:1 with the mass ratio of carbon black after oxidation processes,
Described sodium sulfocyanate accounts for 3.0 ~ 5.0% of this black water mill base gross mass,
Described cosolvent accounts for 3.0 ~ 10.0% of this black water mill base gross mass,
Described bactericide accounts for 0.05 ~ 0.2% of this black water mill base gross mass,
Surplus is deionized water;
Wherein said dispersant is mixed for 1:2 ~ 5 in mass ratio by sodium butylnaphthalenesulfonate salt and 2-naphthalene sulfonic acid formaldehyde polymer sodium salt, and this dispersant system is compared as dispersant with traditional only use 2-naphthalene sulfonic acid formaldehyde polymer sodium salt has better stability.
Its further technical scheme is:
Described carbon black after oxidation processes is for adopting ozone gas to carry out oxidation in the presence of water, oxidant, and in hydroxide and after, reach after filtration the carbon black of dry gained, described oxidant is a kind of in sodium peroxydisulfate, clorox and the hydrogen peroxide, and described hydroxide is a kind of in potassium hydroxide and the NaOH.The used carbon black after oxidation processes of the present invention, on concrete oxidation technology, after carbon black fully disperseed in the aqueous solution, when using oxidizing carbon black through ozone, add a kind of in a small amount of sodium peroxydisulfate, clorox and the hydrogen peroxide and can significantly improve the carbon blacksurface oxidation effectiveness as oxidant, a kind of in recycling potassium hydroxide and the NaOH regulates carbon black pH to 7 after the oxidation ~ about 8, then reach after filtration drying, can obtain the carbon black after the oxidation processes, this carbon black has better easily disperse and anti-reunion performance.
Described surface of pigments finishing agent is a kind of in γ-aminopropyltrimethoxysilane and the APTES.
Described cosolvent is at least a in ethylene glycol, propylene glycol and the glycerine.
Described bactericide is at least a in MIT, BIT and the CMIT, can avoid this black water mill base store and transportation in occur to degrade and go mouldy.
Wherein the use of sodium sulfocyanate is conducive to increase the compatibility of black water mill base and spinning solution.
The present invention also provides the preparation method of a kind of acrylic fibers original liquid coloring with the black water mill base, may further comprise the steps:
(1) in kneader, mediating 0.5～1 hour through the carbon black after the oxidation processes surface of pigments finishing agent and described 20.0 ~ 40.0wt.%;
(2) sodium sulfocyanate with dispersant and described 3.0 ~ 5.0 wt.% is dissolved in the cosolvent and surplus deionized water of 3.0 ~ 10.0wt.%, and disperses 15 ~ 20min with 500 ~ 800r/min rotating speed in dispersion machine, obtains premix;
(3) dispersing speed is down to 300 ~ 400r/min, the carbon black of gained after mediating in (1) added in the premix of gained in (2), under the rotating speed of 1500 ~ 2000r/min, disperseed 0.5 ~ 1 hour, get the charcoal blacks pre-dispersed liquid;
(4) (3) gained charcoal blacks pre-dispersed liquid is carried out continuously grinding 1 ~ 5 hour in horizontal mill, before grinding end, add the bactericide of 0.05 ~ 0.2wt.% half an hour, through deaeration, filtration, obtain the black water mill base for the acrylic fibers original liquid coloring;
Wherein said surface of pigments finishing agent is 0.02 ~ 0.04:1 with the mass ratio of carbon black after oxidation processes, described dispersant is 0.1 ~ 0.3:1 with the mass ratio of carbon black after oxidation processes, and the percentage composition of described carbon black, sodium sulfocyanate, bactericide and cosolvent after oxidation processes is the percentage composition that accounts for this black water mill base gross mass.
Useful technique effect of the present invention is: it is pigment that this acrylic fibers original liquid coloring adopts the carbon black after oxidation processes with the black water mill base, improved the poor shortcoming of ordinary carbon black surface hydrophilicity, and be used in conjunction with sodium butylnaphthalenesulfonate salt and 2-naphthalene sulfonic acid formaldehyde polymer sodium salt composite dispersing agent system, this acrylic fibers original liquid coloring of gained with the black water mill base have particle diameter little, in Polyacrylonitrile Fiber Spinning Solution the high characteristics of stability, spinneret orifice and the larger phenomenon of aberration can not appear during spinning stopping up.
The specific embodiment
Below in conjunction with specific embodiment and comparative example outstanding advantages of the present invention and distinguishing feature are described further, but the present invention is not limited to following embodiment.NM method of operating and method of testing are technology as well known to those skilled in the art among following embodiment and the comparative example.
Embodiment 1
The present embodiment is carbon black oxidation embodiment.With 1000g carbon black and 5000g deionized water, the 50g hydrogen peroxide speed dispersed with stirring 30min with 5r/min in reactor, provide 3% ozone mass concentration, 5L/min speed to enter reactor from the bottom with ozone generator, after processing 5h, sodium hydroxide solution with 10% concentration is regulated pH value to 7.5, filters, dries.
Embodiment 2
The present embodiment is carbon black oxidation embodiment.With 800g carbon black and 5000g deionized water, the 20g sodium peroxydisulfate speed dispersed with stirring 1h with 5r/min in reactor, provide 3% ozone mass concentration, 5L/min speed to enter reactor from the bottom with ozone generator, after processing 3h, potassium hydroxide solution with 15% concentration is regulated pH value to 7.2, filters, dries.
Embodiment 3
The present embodiment is carbon black oxidation embodiment.With 500g carbon black and 5000g deionized water, the 25g clorox speed dispersed with stirring 45min with 5r/min in reactor, provide 3% ozone mass concentration, 5L/min speed to enter reactor from the bottom with ozone generator, after processing 2h, potassium hydroxide solution with 20% concentration is regulated pH value to 8.0, filters, dries.
Embodiment 4～6 and comparative example 7～10 all produce according to following processing step:
(1) will in kneader, mediate 0.5 ~ 1 hour through the carbon black after the oxidation and surface of pigments finishing agent;
(2) dispersant and sodium sulfocyanate are dissolved in cosolvent and the deionized water, and in dispersion machine, disperse 15 ~ 20min with 500 ~ 800r/min rotating speed, obtain premix;
(3) dispersing speed is down to 300 ~ 400r/min, the carbon black after mediating in (1) is added in the premix of gained in (2), under the rotating speed of 1500 ~ 2000r/min, disperseed 0.5 ~ 1 hour, get the charcoal blacks pre-dispersed liquid;
(4) (3) gained charcoal blacks pre-dispersed liquid was carried out continuously grinding 1 ~ 5 hour in horizontal mill, add bactericide half an hour before grinding end, through deaeration, filtration, obtains the black water mill base for the acrylic fibers original liquid coloring.
Embodiment 4～6 and comparative example's 7～10 prescription is as shown in table 1, wherein, MIT represents MIT, BIT represents 1,2-benzisothiazole-3-ketone, CIT represent CMIT, the amount of supplying of described deionized water refers to that it is 100% that the prescription that will be comprised of each component complements to mass fraction, and middle finger of the present invention complements to 100 parts with the prescription that each component forms.
Table 1. embodiment 4～6 and comparative example's 7～10 prescriptions
Mill base performance and application testing
Embodiment 4～6 and comparative example 7～10 all test mill base performance and effect in accordance with the following methods, and test result sees Table 2.
(1) particle diameter distribution tests
The particle diameter of testing above-mentioned black water mill base with Zetasizer Nano Zs90 type nano particle size and the zeta potential instrument of Britain Ma Erwen Instr Ltd. distributes, in the test result, D50 represents that 50% passes through particle diameter, namely survey in the particle minimum grain size that 50% particle can both pass through, in like manner, D99 represents the minimum grain size that 99% particle can both pass through, the particle size that can test the black water mill base with D50, D99.
(2) spinnability test
After the acrylic fibers original liquid coloring of getting respectively 5kg embodiment 4～6 and comparative example 7～10 preparations mixes with the raw material of black water mill base and Polyacrylonitrile Fiber Spinning Solution composition 100kg, its spinneret orifice by 0.08 millimeter in 30 holes is carried out spinning, spinning speed is 30m/min, continuous spinning 24 hours is observed the situation of stopping up spinneret orifice that has or not.
(3) chromatism test
According to the mensuration general rule of standard GB/T 8424.1 textile color stability testing surface colors, objective ranking method and the GB/T 8424.3-2001 textile color stability test Colorimetry that GB/T 8424.2-2001 textile color stability is tested relative whiteness, in the spinnability test process, get respectively the acrylic fiber that spinning began 0.5 hour, 4 hours and prepared in 24 hours, contrast latter two acrylic fibers sample to the aberration of 0.5 hour acrylic fibers sample of spinning.
Table 2 embodiment 4～6 and comparative example's 7～10 test results
Claims (7)
1. an acrylic fibers original liquid coloring black water mill base is characterized in that: be comprised of the carbon black after oxidation processes, surface of pigments finishing agent, dispersant, cosolvent, sodium sulfocyanate, bactericide and deionized water, wherein
Described carbon black after oxidation processes accounts for 20.0 ~ 40.0% of this black water mill base gross mass,
Described surface of pigments finishing agent is 0.02 ~ 0.04:1 with the mass ratio of carbon black after oxidation processes,
Described dispersant is 0.1 ~ 0.3:1 with the mass ratio of carbon black after oxidation processes,
Described sodium sulfocyanate accounts for 3.0 ~ 5.0% of this black water mill base gross mass,
Described cosolvent accounts for 3.0 ~ 10.0% of this black water mill base gross mass,
Described bactericide accounts for 0.05 ~ 0.2% of this black water mill base gross mass,
Surplus is deionized water;
Wherein said dispersant is mixed for 1:2 ~ 5 in mass ratio by sodium butylnaphthalenesulfonate salt and 2-naphthalene sulfonic acid formaldehyde polymer sodium salt.
2. acrylic fibers original liquid coloring black water mill base according to claim 1, it is characterized in that: described carbon black after oxidation processes is for adopting ozone gas to carry out oxidation in the presence of water, oxidant, and in hydroxide and after, reach after filtration the carbon black of dry gained.
3. acrylic fibers original liquid coloring black water mill base according to claim 2 is characterized in that: described oxidant is a kind of in sodium peroxydisulfate, clorox and the hydrogen peroxide, and described hydroxide is a kind of in potassium hydroxide and the NaOH.
4. acrylic fibers original liquid coloring black water mill base according to claim 1 is characterized in that: described surface of pigments finishing agent is a kind of in γ-aminopropyltrimethoxysilane and the APTES.
5. acrylic fibers original liquid coloring black water mill base according to claim 1 is characterized in that: described cosolvent is at least a in ethylene glycol, propylene glycol and the glycerine.
6. acrylic fibers original liquid coloring black water mill base according to claim 1, it is characterized in that: described bactericide is at least a in MIT, BIT and the CMIT.
7. according to the preparation method of the described acrylic fibers original liquid coloring of above arbitrary claim with the black water mill base, it is characterized in that: may further comprise the steps:
(1) in kneader, mediating 0.5～1 hour through the carbon black after the oxidation processes surface of pigments finishing agent and described 20.0 ~ 40.0wt.%;
(2) sodium sulfocyanate with dispersant and described 3.0 ~ 5.0 wt.% is dissolved in the cosolvent and surplus deionized water of 3.0 ~ 10.0wt.%, and disperses 15 ~ 20min with 500 ~ 800r/min rotating speed in dispersion machine, obtains premix;
(3) dispersing speed is down to 300 ~ 400r/min, the carbon black of gained after mediating in (1) added in the premix of gained in (2), under the rotating speed of 1500 ~ 2000r/min, disperseed 0.5 ~ 1 hour, get the charcoal blacks pre-dispersed liquid;
(4) (3) gained charcoal blacks pre-dispersed liquid is carried out continuously grinding 1 ~ 5 hour in horizontal mill, before grinding end, add the bactericide of 0.05 ~ 0.2wt.% half an hour, through deaeration, filtration, obtain the black water mill base for the acrylic fibers original liquid coloring;
Wherein said surface of pigments finishing agent is 0.02 ~ 0.04:1 with the mass ratio of carbon black after oxidation processes, described dispersant is 0.1 ~ 0.3:1 with the mass ratio of carbon black after oxidation processes, and the percentage composition of described carbon black, sodium sulfocyanate, bactericide and cosolvent after oxidation processes is the percentage composition that accounts for this black water mill base gross mass.
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| CN105369385A (en) * | 2014-08-26 | 2016-03-02 | 中国石油化工股份有限公司 | Stock solution coloring acrylic fibers having high color fastness and preparation method |
| CN105463601A (en) * | 2014-08-26 | 2016-04-06 | 中国石油化工股份有限公司 | Acrylic pigment slurry, preparation method and application thereof |
| CN106398306A (en) * | 2016-08-26 | 2017-02-15 | 苏州世名科技股份有限公司 | Pigment preparing product used for acrylon stock solution dying, and preparation method thereof |
| CN107587204A (en) * | 2017-09-25 | 2018-01-16 | 浙江纳美新材料股份有限公司 | A kind of polyimides stoste colouring pigments dispersion and preparation method thereof |
| CN110964349A (en) * | 2018-09-30 | 2020-04-07 | 山东欧铂新材料有限公司 | Oxidation modified carbon black and preparation method thereof |
| CN111155187A (en) * | 2020-01-19 | 2020-05-15 | 浙江纳美新材料股份有限公司 | Conductive black water-based color paste for coloring viscose stock solution and preparation method thereof |
| CN111171607A (en) * | 2020-04-09 | 2020-05-19 | 北京化工大学 | Method for preparing hydrophilic carbon black, hydrophilic carbon black and application thereof |
| CN112410915A (en) * | 2019-08-23 | 2021-02-26 | 中国石油化工股份有限公司 | Coloring paste suitable for dry acrylic fibers and application thereof |
| CN113801520A (en) * | 2021-08-23 | 2021-12-17 | 明光科迪新材料有限公司 | Nano color paste for water-based UV plastic paint and preparation method thereof |
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| CN105463601A (en) * | 2014-08-26 | 2016-04-06 | 中国石油化工股份有限公司 | Acrylic pigment slurry, preparation method and application thereof |
| CN105369385B (en) * | 2014-08-26 | 2019-08-13 | 中国石油化工股份有限公司 | A kind of Dope Dyed Acrylic Fiber and preparation method with high color fastness |
| CN105369385A (en) * | 2014-08-26 | 2016-03-02 | 中国石油化工股份有限公司 | Stock solution coloring acrylic fibers having high color fastness and preparation method |
| CN106398306B (en) * | 2016-08-26 | 2017-12-29 | 苏州世名科技股份有限公司 | Pigment preparation matter for acrylic fibers original liquid coloring and preparation method thereof |
| CN106398306A (en) * | 2016-08-26 | 2017-02-15 | 苏州世名科技股份有限公司 | Pigment preparing product used for acrylon stock solution dying, and preparation method thereof |
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| CN110964349A (en) * | 2018-09-30 | 2020-04-07 | 山东欧铂新材料有限公司 | Oxidation modified carbon black and preparation method thereof |
| CN110964349B (en) * | 2018-09-30 | 2021-08-17 | 山东欧铂新材料有限公司 | Oxidation modified carbon black and preparation method thereof |
| CN112410915A (en) * | 2019-08-23 | 2021-02-26 | 中国石油化工股份有限公司 | Coloring paste suitable for dry acrylic fibers and application thereof |
| CN112410915B (en) * | 2019-08-23 | 2022-08-12 | 中国石油化工股份有限公司 | Coloring paste suitable for dry acrylic fibers and application thereof |
| CN111155187A (en) * | 2020-01-19 | 2020-05-15 | 浙江纳美新材料股份有限公司 | Conductive black water-based color paste for coloring viscose stock solution and preparation method thereof |
| CN111171607A (en) * | 2020-04-09 | 2020-05-19 | 北京化工大学 | Method for preparing hydrophilic carbon black, hydrophilic carbon black and application thereof |
| CN111171607B (en) * | 2020-04-09 | 2021-05-04 | 北京化工大学 | Method for preparing hydrophilic carbon black, hydrophilic carbon black and application thereof |
| CN113801520A (en) * | 2021-08-23 | 2021-12-17 | 明光科迪新材料有限公司 | Nano color paste for water-based UV plastic paint and preparation method thereof |
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